CN117285993A - Laundry effervescent tablet and preparation method thereof - Google Patents
Laundry effervescent tablet and preparation method thereof Download PDFInfo
- Publication number
- CN117285993A CN117285993A CN202311193207.0A CN202311193207A CN117285993A CN 117285993 A CN117285993 A CN 117285993A CN 202311193207 A CN202311193207 A CN 202311193207A CN 117285993 A CN117285993 A CN 117285993A
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- Prior art keywords
- parts
- sucrose
- acid
- temperature
- solution
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- 239000007938 effervescent tablet Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000004005 microsphere Substances 0.000 claims abstract description 99
- 238000005406 washing Methods 0.000 claims abstract description 64
- 239000002245 particle Substances 0.000 claims abstract description 52
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 38
- 102000004190 Enzymes Human genes 0.000 claims abstract description 22
- 108090000790 Enzymes Proteins 0.000 claims abstract description 22
- 230000001954 sterilising effect Effects 0.000 claims abstract description 19
- 239000000853 adhesive Substances 0.000 claims abstract description 15
- 230000001070 adhesive effect Effects 0.000 claims abstract description 15
- 239000003755 preservative agent Substances 0.000 claims abstract description 10
- 230000002335 preservative effect Effects 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 229930006000 Sucrose Natural products 0.000 claims description 120
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 120
- 239000005720 sucrose Substances 0.000 claims description 120
- 239000000243 solution Substances 0.000 claims description 116
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 71
- 238000003756 stirring Methods 0.000 claims description 68
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 54
- 238000009210 therapy by ultrasound Methods 0.000 claims description 53
- 150000007524 organic acids Chemical class 0.000 claims description 37
- 150000003445 sucroses Chemical class 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 claims description 26
- 239000000839 emulsion Substances 0.000 claims description 26
- 239000011259 mixed solution Substances 0.000 claims description 24
- MUPFEKGTMRGPLJ-RMMQSMQOSA-N Raffinose Natural products O(C[C@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@@H](O[C@@]2(CO)[C@H](O)[C@@H](O)[C@@H](CO)O2)O1)[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 MUPFEKGTMRGPLJ-RMMQSMQOSA-N 0.000 claims description 22
- MUPFEKGTMRGPLJ-UHFFFAOYSA-N UNPD196149 Natural products OC1C(O)C(CO)OC1(CO)OC1C(O)C(O)C(O)C(COC2C(C(O)C(O)C(CO)O2)O)O1 MUPFEKGTMRGPLJ-UHFFFAOYSA-N 0.000 claims description 22
- MUPFEKGTMRGPLJ-ZQSKZDJDSA-N raffinose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO[C@@H]2[C@@H]([C@@H](O)[C@@H](O)[C@@H](CO)O2)O)O1 MUPFEKGTMRGPLJ-ZQSKZDJDSA-N 0.000 claims description 22
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 21
- 229940088598 enzyme Drugs 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 18
- 239000013078 crystal Substances 0.000 claims description 16
- 238000002425 crystallisation Methods 0.000 claims description 16
- 230000008025 crystallization Effects 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 14
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical group [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 13
- 235000020661 alpha-linolenic acid Nutrition 0.000 claims description 13
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- 229920000742 Cotton Polymers 0.000 claims description 11
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 11
- 102000005840 alpha-Galactosidase Human genes 0.000 claims description 11
- 108010030291 alpha-Galactosidase Proteins 0.000 claims description 11
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- 238000001914 filtration Methods 0.000 claims description 11
- 238000004090 dissolution Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 108091005658 Basic proteases Proteins 0.000 claims description 8
- 229920002785 Croscarmellose sodium Polymers 0.000 claims description 8
- 235000010947 crosslinked sodium carboxy methyl cellulose Nutrition 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 7
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 7
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 7
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- 229960001681 croscarmellose sodium Drugs 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
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- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 7
- 239000011975 tartaric acid Substances 0.000 claims description 7
- 235000002906 tartaric acid Nutrition 0.000 claims description 7
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- YZXBAPSDXZZRGB-DOFZRALJSA-N arachidonic acid Chemical compound CCCCC\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O YZXBAPSDXZZRGB-DOFZRALJSA-N 0.000 claims description 6
- 239000003899 bactericide agent Substances 0.000 claims description 6
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 claims description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-MDZDMXLPSA-N elaidic acid Chemical compound CCCCCCCC\C=C\CCCCCCCC(O)=O ZQPPMHVWECSIRJ-MDZDMXLPSA-N 0.000 claims description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 6
- 229940057950 sodium laureth sulfate Drugs 0.000 claims description 6
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 5
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 4
- 229920002472 Starch Polymers 0.000 claims description 4
- 235000015165 citric acid Nutrition 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000008107 starch Substances 0.000 claims description 4
- 235000019698 starch Nutrition 0.000 claims description 4
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 4
- BITHHVVYSMSWAG-KTKRTIGZSA-N (11Z)-icos-11-enoic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCC(O)=O BITHHVVYSMSWAG-KTKRTIGZSA-N 0.000 claims description 3
- GWHCXVQVJPWHRF-KTKRTIGZSA-N (15Z)-tetracosenoic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCCCC(O)=O GWHCXVQVJPWHRF-KTKRTIGZSA-N 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- JBYXPOFIGCOSSB-GOJKSUSPSA-N 9-cis,11-trans-octadecadienoic acid Chemical compound CCCCCC\C=C\C=C/CCCCCCCC(O)=O JBYXPOFIGCOSSB-GOJKSUSPSA-N 0.000 claims description 3
- DPUOLQHDNGRHBS-UHFFFAOYSA-N Brassidinsaeure Natural products CCCCCCCCC=CCCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-UHFFFAOYSA-N 0.000 claims description 3
- URXZXNYJPAJJOQ-UHFFFAOYSA-N Erucic acid Natural products CCCCCCC=CCCCCCCCCCCCC(O)=O URXZXNYJPAJJOQ-UHFFFAOYSA-N 0.000 claims description 3
- OPGOLNDOMSBSCW-CLNHMMGSSA-N Fursultiamine hydrochloride Chemical compound Cl.C1CCOC1CSSC(\CCO)=C(/C)N(C=O)CC1=CN=C(C)N=C1N OPGOLNDOMSBSCW-CLNHMMGSSA-N 0.000 claims description 3
- XJXROGWVRIJYMO-SJDLZYGOSA-N Nervonic acid Natural products O=C(O)[C@@H](/C=C/CCCCCCCC)CCCCCCCCCCCC XJXROGWVRIJYMO-SJDLZYGOSA-N 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- JAZBEHYOTPTENJ-JLNKQSITSA-N all-cis-5,8,11,14,17-icosapentaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O JAZBEHYOTPTENJ-JLNKQSITSA-N 0.000 claims description 3
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- GWHCXVQVJPWHRF-UHFFFAOYSA-N cis-tetracosenoic acid Natural products CCCCCCCCC=CCCCCCCCCCCCCCC(O)=O GWHCXVQVJPWHRF-UHFFFAOYSA-N 0.000 claims description 3
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- DPUOLQHDNGRHBS-KTKRTIGZSA-N erucic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-KTKRTIGZSA-N 0.000 claims description 3
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 claims description 3
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- WCKIDCVWRJUPFY-UHFFFAOYSA-L zinc;oxalate;dihydrate Chemical compound O.O.[Zn+2].[O-]C(=O)C([O-])=O WCKIDCVWRJUPFY-UHFFFAOYSA-L 0.000 claims description 3
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- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 2
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D10/00—Compositions of detergents, not provided for by one single preceding group
- C11D10/04—Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap
- C11D10/042—Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap based on anionic surface-active compounds and soap
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0047—Detergents in the form of bars or tablets
- C11D17/0065—Solid detergents containing builders
- C11D17/0073—Tablets
- C11D17/0086—Laundry tablets
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/29—Sulfates of polyoxyalkylene ethers
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Abstract
The invention discloses a laundry effervescent tablet and a preparation method thereof, wherein the laundry effervescent tablet comprises the following raw materials: washing particles, microsphere inclusion, sterilizing preservative, disintegrating agent, enzyme, effervescent agent and adhesive. The washing effervescent tablet prepared by the invention has good washing effect and strong decontamination capability, and can also effectively prevent the occurrence of clothes dyeing in the washing process.
Description
Technical Field
The invention belongs to the technical field of daily chemical washing products, and particularly relates to a laundry effervescent tablet and a preparation method thereof.
Background
Compared with common washing products such as washing powder, washing soap, liquid detergent and the like, the washing tablet is formed by mixing and pressing powdery washing agent and tablet forming auxiliary agent, and is more convenient to carry and more accurate in metering. The effervescent tablet is a kind of washing tablet, which is named as effervescent tablet by using the reaction of organic acid and basic bicarbonate (hydrogen) as effervescent disintegrant, and after being put into water, the effervescent tablet produces a great amount of carbon dioxide, and the state of the effervescent tablet is boiling. The effervescent tablet disintegrates to generate a great amount of foam, which increases the direct contact between the surfactant and clothes, and has better washing effect. Chinese patent CN105238604A discloses a high-stability salt-containing laundry effervescent tablet and a preparation method thereof, wherein the tablet is prepared by the following processes of mixing, granulating, tabletting, film coating and the like of a raw material nonionic surfactant, an anionic surfactant, a washing auxiliary agent, sodium chloride, an adhesive, an effervescent agent, a coating agent, ethylene diamine tetraacetic acid tetrasodium salt and a lubricant.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a laundry effervescent tablet and a preparation method thereof.
A method for preparing a laundry effervescent tablet, comprising the following steps:
according to parts by weight, 20 to 40 parts of washing particles, 4 to 8 parts of microsphere inclusion, 0.5 to 5 parts of disintegrating agent, 0.4 to 0.6 part of enzyme, 30 to 50 parts of effervescent agent and 15 to 25 parts of adhesive are mixed at a rotating speed of 200 to 400r/min and stirred for 20 to 40min, and then extruded on a die to form a sheet with a diameter of 1.5 to 3cm and a thickness of 0.4 to 0.6cm, so as to obtain the laundry effervescent tablet.
Preferably, a method for preparing the laundry effervescent tablet comprises the following steps:
according to parts by weight, 20 to 40 parts of washing particles, 4 to 8 parts of microsphere inclusion bodies, 1 to 4 parts of sterilizing preservative, 0.5 to 5 parts of disintegrating agent, 0.4 to 0.6 part of enzyme, 30 to 50 parts of effervescent agent and 15 to 25 parts of adhesive are mixed at a rotating speed of 200 to 400r/min and stirred for 20 to 40min, and then extruded on a die into a sheet with a diameter of 1.5 to 3cm and a thickness of 0.4 to 0.6cm, so that the laundry effervescent tablet is obtained.
The disintegrating agent is one or more of crosslinked sodium carboxymethyl cellulose, crosslinked povidone, starch, sodium carboxymethyl starch, hydroxypropyl starch and low-substituted hydroxypropyl cellulose. Preferably, the disintegrant is croscarmellose sodium.
The enzyme is one or more of alkaline protease, pectase, cellulase, lipase and catalase. Preferably, the enzyme is an alkaline protease.
The effervescent agent is a combination of an acid source and an alkali source. The acid source is one or more of citric acid, malic acid, boric acid, tartaric acid, fumaric acid and inorganic mineral acid. The alkali source is sodium bicarbonate or sodium carbonate or a mixture of the two. Preferably, the effervescent agent is a mixture of sodium bicarbonate and tartaric acid according to a mass ratio of (1-2): 1.
The adhesive is absolute ethyl alcohol or water. Preferably, the binder is absolute ethanol.
The preparation method of the washing particles comprises the following steps:
(1) Adding 10-25 parts by weight of sodium dodecyl benzene sulfonate and 10-25 parts by weight of sodium laureth sulfate into 60-120 parts by weight of water, heating to 75-90 ℃, and stirring for 20-40 min at a rotating speed of 500-700 r/min to obtain a mixed solution A;
(2) According to parts by weight, when 80-120 parts of the mixed solution A obtained in the step (1) is naturally cooled to 30-40 ℃, 3-5 parts of sodium stearate, 4-6 parts of glycerol cocoate and 1-3 parts of sodium chloride are added, the temperature is kept at 30-40 ℃ and the rotation speed is 500-700 r/min, and stirring is carried out for 30-50 min, so as to obtain a mixed solution B;
(3) Granulating the mixed solution B obtained in the step (2) by a spray granulator to obtain particles with the particle size of 0.1-0.3 mm, and drying the particles for 8-12 h at the temperature of 50-70 ℃ by an oven to obtain the washing particles.
The preparation method of the microsphere inclusion comprises the following steps:
s1, preparing a sucrose supersaturated solution: adding sucrose into water according to parts by weight, wherein the dissolution temperature is 20-80 ℃, stirring for 15-30 min at the rotation speed of 500-700 r/min to form a sucrose supersaturated solution, and determining the solubility of the sucrose and the water at the selected dissolution temperature according to the mass ratio of the sucrose to the water to prepare the sucrose supersaturated solution with the supersaturation degree of 1.06-1.1;
s2, ultrasonic treatment: carrying out ultrasonic treatment on the sucrose supersaturated solution obtained in the step S1 for 20-40 min, wherein the ultrasonic temperature is controlled to be 20-80 ℃, the ultrasonic power is 80-120W, and the ultrasonic frequency is 20-40 kHz, so as to obtain the sucrose supersaturated solution after ultrasonic treatment;
s3, removing cotton sugar: adding 0.1-0.3 part of alpha-galactosidase into 20-40 parts of supersaturated sucrose solution obtained in the step S2 after ultrasonic treatment, stirring for 15-30 min at the temperature of 20-80 ℃ and the rotating speed of 500-700 r/min to obtain supersaturated sucrose solution after removing raffinose;
s4, forming sucrose microspheres: adding 1-3 parts by weight of epichlorohydrin into 20-30 parts by weight of supersaturated sucrose solution obtained in the step S3 after removing the raffinose, and stirring for 8-12 min at a rotating speed of 200-400 r/min to form a water phase A; adding 2-4 parts of span 80 into 4-6 parts of liquid paraffin, and stirring for 15-25 min at a rotating speed of 200-400 r/min to obtain an oil phase B; adding 4-6 parts of oil phase B into 20-30 parts of water phase A at a rate of 1 drop/second, stirring at a temperature of 35-50 ℃ and a rotating speed of 800-1000 r/min for 1.5-3.0 h to form uniform emulsion C, adding 0.5-1.5 parts of glutaraldehyde into 20-35 parts of emulsion C, standing at a temperature of 35-50 ℃ for 1-3 h to obtain a mixed sugar solution containing sucrose microspheres, filtering and washing the mixed sugar solution containing sucrose microspheres with water, and freeze-drying at a temperature of-20 to-25 ℃ for 3-5 h to obtain microsphere inclusion.
Preferably, the preparation method of the microsphere inclusion comprises the following steps:
s1, preparing a sucrose supersaturated solution: adding sucrose into water according to parts by weight, wherein the dissolution temperature is 20-80 ℃, stirring for 15-30 min at the rotation speed of 500-700 r/min to form a sucrose supersaturated solution, and determining the solubility of the sucrose and the water at the selected dissolution temperature according to the mass ratio of the sucrose to the water to prepare the sucrose supersaturated solution with the supersaturation degree of 1.06-1.1;
s2, ultrasonic treatment: carrying out ultrasonic treatment on the sucrose supersaturated solution obtained in the step S1 for 20-40 min, wherein the ultrasonic temperature is controlled to be 20-80 ℃, the ultrasonic power is 80-120W, and the ultrasonic frequency is 20-40 kHz, so as to obtain the sucrose supersaturated solution after ultrasonic treatment;
s3, removing cotton sugar: adding 0.1-0.3 part of alpha-galactosidase into 20-40 parts of supersaturated sucrose solution obtained in the step S2 after ultrasonic treatment, stirring for 15-30 min at the temperature of 20-80 ℃ and the rotating speed of 500-700 r/min to obtain supersaturated sucrose solution after removing raffinose;
s4, forming sucrose microspheres: adding 1-3 parts by weight of epichlorohydrin into 20-30 parts by weight of supersaturated sucrose solution obtained in the step S3 after removing the raffinose, and stirring for 8-12 min at a rotating speed of 200-400 r/min to form a water phase A; adding 2-4 parts of span 80 into 4-6 parts of liquid paraffin, and stirring for 15-25 min at a rotating speed of 200-400 r/min to obtain an oil phase B; dripping 0.1-0.3 part of organic acid and 4-6 parts of oil phase B into 20-30 parts of water phase A at the speed of 1 drop/second respectively, stirring at the temperature of 35-50 ℃ and the rotating speed of 800-1000 r/min for 1.5-3.0 h to form uniform emulsion C, adding 0.5-1.5 part of glutaraldehyde into 20-35 parts of emulsion C, standing for 1-3 h at the temperature of 35-50 ℃ to obtain mixed sugar solution containing sucrose microspheres, filtering and washing the mixed sugar solution containing sucrose microspheres with water, and freeze-drying at the temperature of-20 to-25 ℃ for 3-5 h to obtain microsphere inclusion.
The invention adopts an emulsion crosslinking method to prepare sucrose microspheres, supersaturated sucrose solution and epichlorohydrin molecules are mixed together, the supersaturated sucrose solution and epichlorohydrin molecules are mixed with oil phase medium in a droplet form under the action of stirring shearing force to form emulsion, a small polymerization unit is formed in the aqueous phase droplet, highly crosslinked particles are generated by sucrose molecules and epichlorohydrin molecules along with the continuous reaction, glutaraldehyde and organic acid are added into the emulsion at the moment, aldehyde groups in glutaraldehyde can be subjected to condensation reaction with hydroxyl groups of sucrose, the formed bridge bonds can solidify the microspheres, the organic acid is fixed in microsphere frameworks, the honeycomb network structure of the microsphere frameworks can well wrap the organic acid, and the microsphere frameworks not only can absorb pigments in aqueous solution, but also can help to protect the activity of enzymes and promote the removal effect of enzymes on stains. At the moment, the temperature of supersaturated sucrose mother solution is reduced, rapid crystallization is carried out, meanwhile, the formation of the sucrose microsphere skeleton can also accelerate the crystallization process, and the microsphere skeleton is further wrapped during sucrose crystallization, so that the effervescent agent in the effervescent tablet reacts on organic acid. When washing clothes, the effervescent tablet is dissolved in water, the acid source and the alkali source in the effervescent agent react rapidly, the sucrose crystals are released in the water solution, the microsphere frameworks are released after the sucrose crystals are dissolved in the water, the organic acid is dissolved in the water solution, at the moment, the multi-void structure in the microsphere frameworks has electrostatic adsorption effect on free dye particles, the free dye particles can be firmly wrapped, the free dye particles are prevented from dying other clothes, and the dyeing prevention effect is achieved.
After the washing effervescent tablet is dissolved in water, the alkalinity is stronger, the stronger alkaline environment is not beneficial to the electrostatic adsorption effect of the microsphere frameworks on free dye particles, organic acid is added to the effervescent tablet, wherein citric acid has an adjusting effect on the pH of the washing environment, when the pH of the washing aqueous solution gradually decreases, the surface charge density of the microsphere frameworks is increased due to the deprotonation effect, the electrostatic effect of the free dye liquid between the microsphere frameworks is increased, and the removal rate of the free dye particles is increased; meanwhile, citric acid can help the microsphere framework to loosen pore channels, increase the average pore diameter and improve the adsorption effect of the microsphere framework on free pigment; the alpha-linolenic acid can help the clothes to protect the color, reduce the damage of the polarity of water to the intermolecular action of the dye, increase the fixation of the dye on the surface of the fabric, reduce the dropping of the color of the fabric, and the citric acid and the alpha-linolenic acid are compounded, so that the free pigment particles dropped from the clothes can be adsorbed by the microsphere framework while the dropping of the clothes is reduced as much as possible, the dyeing of the light-colored clothes by the free pigment in the water is avoided, and the washed fabric has the effects of protecting the color and preventing dyeing.
The washing particles, microsphere inclusion bodies and other auxiliary materials are made into effervescent tablets, and the effervescent tablets can generate a large amount of carbon dioxide at the moment of meeting water, so that the penetration of water and surfactant in fabrics is assisted, and the clothes are washed faster, cleaner and more thoroughly.
Further preferably, the preparation method of the microsphere inclusion comprises the following steps:
s1, preparing a sucrose supersaturated solution: adding sucrose into water according to parts by weight, wherein the dissolution temperature is 20-80 ℃, stirring for 15-30 min at the rotation speed of 500-700 r/min to form a sucrose supersaturated solution, and determining the solubility of the sucrose and the water at the selected dissolution temperature according to the mass ratio of the sucrose to the water to prepare the sucrose supersaturated solution with the supersaturation degree of 1.06-1.1;
s2, ultrasonic treatment: carrying out ultrasonic treatment on the sucrose supersaturated solution obtained in the step S1 for 20-40 min, wherein the ultrasonic temperature is controlled to be 20-80 ℃, the ultrasonic power is 80-120W, and the ultrasonic frequency is 20-40 kHz, so as to obtain the sucrose supersaturated solution after ultrasonic treatment;
s3, removing cotton sugar: adding 0.1-0.3 part of alpha-galactosidase into 20-40 parts of supersaturated sucrose solution obtained in the step S2 after ultrasonic treatment, stirring for 15-30 min at the temperature of 20-80 ℃ and the rotating speed of 500-700 r/min to obtain supersaturated sucrose solution after removing raffinose;
s4, forming sucrose microspheres: adding 1-3 parts by weight of epichlorohydrin into 20-30 parts by weight of supersaturated sucrose solution obtained in the step S3 after removing the raffinose, and stirring for 8-12 min at a rotating speed of 200-400 r/min to form a water phase A; adding 2-4 parts of span 80 into 4-6 parts of liquid paraffin, and stirring for 15-25 min at a rotating speed of 200-400 r/min to obtain an oil phase B; dripping 0.1-0.3 part of organic acid and 4-6 parts of oil phase B into 20-30 parts of water phase A at the speed of 1 drop/second respectively, stirring at the temperature of 35-50 ℃ and the rotating speed of 800-1000 r/min for 1.5-3.0 h to form uniform emulsion C, adding 0.5-1.5 parts of glutaraldehyde into 20-35 parts of emulsion C, and standing at the temperature of 35-50 ℃ for 1-3 h to obtain the mixed sugar solution containing sucrose microspheres.
S5, crystallization: and (3) transferring 15-25 parts by weight of the mixed sugar solution containing the sucrose microspheres obtained in the step (S4) into a round-bottom flask, placing the round-bottom flask in an ice bath condition, controlling the ice bath temperature to be 0-2 ℃, carrying out low-temperature rapid crystallization for 20-40 min at the rotating speed of 500-700 r/min, filtering, and drying the crystal in an oven at 50-70 ℃ for 6-10 h to obtain the microsphere inclusion.
The organic acid is one or more of citric acid, alpha-linolenic acid, stearidonic acid, eicosapentaenoic acid, conjugated linoleic acid, gamma-linoleic acid, arachidonic acid, oleic acid, trans-oleic acid, eicosenoic acid, erucic acid and nervonic acid. Preferably, the organic acid is citric acid and alpha-linolenic acid which are mixed according to the mass ratio of 1 (1.0-1.5).
The sterilizing preservative is formed by mixing inorganic sterilizing substances and dodecyl dimethyl benzyl ammonium chloride according to the mass ratio of 5 (1-3).
The preparation method of the inorganic bactericide comprises the following steps:
adding 2-5 parts of sodium hydroxide into 80-100 parts of mixed alcohol according to parts by weight, and performing ultrasonic treatment for 10-20 min, wherein the ultrasonic temperature is controlled at 30-50 ℃, the ultrasonic power is 100-300W, and the ultrasonic frequency is 20-40 kHz, so as to obtain sodium hydroxide alcohol solution; adding 2-4 parts of zinc oxalate dihydrate into 150-200 parts of mixed alcohol, and performing ultrasonic treatment for 30-50 min, wherein the ultrasonic temperature is controlled at 30-50 ℃, the ultrasonic power is 100-300W, and the ultrasonic frequency is 20-40 kHz; then 20-30 parts of the sodium hydroxide alcohol solution is dripped, and the dripping speed is controlled to be 1-2 mL/min; after the dripping is finished, adding 0.1 to 0.3 part of 3-glycidoxypropyl trimethoxy silane, continuing ultrasonic treatment for 10 to 20 minutes, centrifuging, taking the precipitate, washing the precipitate with water, and drying the precipitate in an oven at 60 to 80 ℃ for 7 to 10 hours to obtain an inorganic bactericide; the mixed alcohol is a mixture of ethanol and glycol according to the mass ratio of 13 (1-2).
The invention has the beneficial effects that: the washing effervescent tablet prepared by the invention has good washing effect and strong decontamination capability, can effectively prevent the occurrence of clothes dyeing in the washing process, and has good sterilization effect. According to the invention, the sucrose microsphere inclusion is prepared by adopting an emulsion crosslinking method, and the organic acid is fixed on the honeycomb net structure of the microsphere framework, so that the organic acid is well wrapped, the microsphere framework not only can adsorb pigments in aqueous solution, but also can help to protect the activity of enzyme and promote the removal of the enzyme on stains. Meanwhile, the formation of the microsphere skeleton of the sucrose can accelerate the crystallization process, and the microsphere skeleton is further wrapped during the sucrose crystallization, so that the effervescent agent in the effervescent tablet is prevented from reacting with organic acid. When washing clothes, the effervescent tablet is dissolved in water, the acid source and the alkali source in the effervescent agent react rapidly, the sucrose crystals are released in the water solution, the microsphere frameworks are released after the sucrose crystals are dissolved in the water, the organic acid is dissolved in the water solution, at the moment, the multi-void structure in the microsphere frameworks has electrostatic adsorption effect on free dye particles, the free dye particles can be firmly wrapped, the free dye particles are prevented from dying other clothes, and the dyeing prevention effect is achieved.
Detailed Description
The raw materials used in the examples are as follows:
sodium laurinol polyoxyethylene ether sulfate, CAS number: 9004-82-4, available from Shenzhen chemical engineering Co., ltd., product number 6001.
Glycerol cocoate, CAS number: 68201-46-7, model number from the wuhan Hua Xiangke biotechnology company, inc: PED-7.
Croscarmellose sodium, purchased from zhengzhou kangyuan chemical products, inc., CAS number: 74811-65-7.
Alkaline protease, CAS number: 9014-01-1, enzyme activity purchased from Anhui Mukang food Co., ltd.: 10 ten thousand U/g.
Liquid paraffin, CAS number: 8042-47-5, density, purchased from Shanghai Alasdine Biotechnology Co., ltd.): 0.86-0.89.
Example 1
The preparation method of the laundry effervescent tablet comprises the following steps:
according to parts by weight, 30 parts of washing particles, 6 parts of microsphere inclusion, 3.5 parts of disintegrating agent, 0.5 part of enzyme, 40 parts of effervescent agent and 20 parts of adhesive are stirred for 30 minutes at a rotating speed of 300r/min, uniformly mixed, and then extruded on a die to form a sheet with a diameter of 2cm and a thickness of 0.5cm, so that the laundry effervescent tablet is obtained.
The disintegrating agent is croscarmellose sodium.
The enzyme is alkaline protease.
The effervescent agent is prepared by mixing sodium bicarbonate and tartaric acid according to a mass ratio of 1:1.
The adhesive is absolute ethyl alcohol.
The preparation method of the washing particles comprises the following steps:
(1) Adding 20 parts of sodium dodecyl benzene sulfonate and 20 parts of sodium laureth sulfate into 100 parts of water, heating to 85 ℃, and stirring at 600r/min for 30min to obtain a mixed solution A;
(2) According to parts by weight, when 100 parts of the mixed solution A obtained in the step (1) is naturally cooled to 35 ℃, 4 parts of sodium stearate, 5 parts of glycerol cocoate and 2 parts of sodium chloride are added, the temperature is kept at 35 ℃ and the rotation speed is 600r/min, and stirring is carried out for 40min, so as to obtain a mixed solution B;
(3) Granulating the mixed solution B obtained in the step (2) by a spray granulator to obtain particles with the particle size of 0.2mm, and then placing the particles in a 60 ℃ oven for drying for 10 hours to obtain the washing particles.
The preparation method of the microsphere inclusion comprises the following steps:
s1, preparing a sucrose supersaturated solution: adding 92 parts by weight of sucrose into 40 parts by weight of water, and stirring at 26 ℃ for 20 minutes at a rotating speed of 600r/min to form a sucrose supersaturated solution;
s2, ultrasonic treatment: carrying out ultrasonic treatment on the sucrose supersaturated solution obtained in the step S1 for 30min, wherein the ultrasonic temperature is controlled at 26 ℃, the ultrasonic power is 100W, and the ultrasonic frequency is 25kHz, so as to obtain the sucrose supersaturated solution after ultrasonic treatment;
s3, removing cotton sugar: adding 0.2 part of alpha-galactosidase into 30 parts of the supersaturated sucrose solution obtained in the step S2 after ultrasonic treatment, and stirring for 20min at 26 ℃ and a rotating speed of 600r/min to obtain a supersaturated sucrose solution after removing the raffinose;
s4, forming sucrose microspheres: adding 2 parts by weight of epichlorohydrin into 25 parts by weight of supersaturated sucrose solution obtained in the step S3 after removing the raffinose, and stirring for 10min at a rotating speed of 300r/min to form a water phase A; adding 3 parts of span 80 into 5 parts of liquid paraffin, and stirring at a rotating speed of 300r/min for 20min to obtain an oil phase B; adding 0.2 part of organic acid and 5 parts of oil phase B into 25 parts of water phase A at a rate of 1 drop/second, stirring at a speed of 900r/min for 2 hours at 40 ℃ to form uniform emulsion C, adding 1 part of glutaraldehyde into 30 parts of emulsion C, standing at 40 ℃ for 2 hours to obtain a mixed sugar solution containing sucrose microspheres, filtering and washing the mixed sugar solution containing sucrose microspheres with water, and freeze-drying at-20 ℃ for 4 hours to obtain microsphere inclusion bodies.
The organic acid is citric acid.
Example 2
Substantially the same as in example 1, the only difference is that:
the preparation method of the microsphere inclusion comprises the following steps:
s1, preparing a sucrose supersaturated solution: adding 92 parts by weight of sucrose into 40 parts by weight of water, and stirring at 26 ℃ for 20 minutes at a rotating speed of 600r/min to form a sucrose supersaturated solution;
s2, ultrasonic treatment: carrying out ultrasonic treatment on the sucrose supersaturated solution obtained in the step S1 for 30min, wherein the ultrasonic temperature is controlled at 26 ℃, the ultrasonic power is 100W, and the ultrasonic frequency is 25kHz, so as to obtain the sucrose supersaturated solution after ultrasonic treatment;
s3, removing cotton sugar: adding 0.2 part of alpha-galactosidase into 30 parts of the supersaturated sucrose solution obtained in the step S2 after ultrasonic treatment, and stirring for 20min at 26 ℃ and a rotating speed of 600r/min to obtain a supersaturated sucrose solution after removing the raffinose;
s4, forming sucrose microspheres: adding 2 parts by weight of epichlorohydrin into 25 parts by weight of supersaturated sucrose solution obtained in the step S3 after removing the raffinose, and stirring for 10min at a rotating speed of 300r/min to form a water phase A; adding 3 parts of span 80 into 5 parts of liquid paraffin, and stirring at a rotating speed of 300r/min for 20min to obtain an oil phase B; dropwise adding 0.2 part of organic acid and 5 parts of oil phase B into 25 parts of water phase A at a rate of 1 drop/second respectively, stirring at 40 ℃ and a rotating speed of 900r/min for 2 hours to form uniform emulsion C, adding 1 part of glutaraldehyde into 30 parts of emulsion C, and standing at 40 ℃ for 2 hours to obtain a mixed sugar solution containing sucrose microspheres;
s5, crystallization: and (3) transferring 20 parts by weight of the mixed sugar solution containing the sucrose microspheres obtained in the step (S4) into a round-bottom flask, placing the round-bottom flask in an ice bath condition, controlling the ice bath temperature to be 2 ℃, carrying out low-temperature rapid crystallization for 30min at the rotating speed of 600r/min, filtering, and drying the crystal in a baking oven at the temperature of 60 ℃ for 10h to obtain the microsphere inclusion.
The organic acid is citric acid.
Example 3
Substantially the same as in example 1, the only difference is that:
the preparation method of the microsphere inclusion comprises the following steps:
s1, preparing a sucrose supersaturated solution: adding 92 parts by weight of sucrose into 40 parts by weight of water, and stirring at 26 ℃ for 20 minutes at a rotating speed of 600r/min to form a sucrose supersaturated solution;
s2, ultrasonic treatment: carrying out ultrasonic treatment on the sucrose supersaturated solution obtained in the step S1 for 30min, wherein the ultrasonic temperature is controlled at 26 ℃, the ultrasonic power is 100W, and the ultrasonic frequency is 25kHz, so as to obtain the sucrose supersaturated solution after ultrasonic treatment;
s3, removing cotton sugar: adding 0.2 part of alpha-galactosidase into 30 parts of the supersaturated sucrose solution obtained in the step S2 after ultrasonic treatment, and stirring for 20min at 26 ℃ and a rotating speed of 600r/min to obtain a supersaturated sucrose solution after removing the raffinose;
s4, forming sucrose microspheres: adding 2 parts by weight of epichlorohydrin into 25 parts by weight of supersaturated sucrose solution obtained in the step S3 after removing the raffinose, and stirring for 10min at a rotating speed of 300r/min to form a water phase A; adding 3 parts of span 80 into 5 parts of liquid paraffin, and stirring at a rotating speed of 300r/min for 20min to obtain an oil phase B; dropwise adding 0.2 part of organic acid and 5 parts of oil phase B into 25 parts of water phase A at a rate of 1 drop/second respectively, stirring at 40 ℃ and a rotating speed of 900r/min for 2 hours to form uniform emulsion C, adding 1 part of glutaraldehyde into 30 parts of emulsion C, and standing at 40 ℃ for 2 hours to obtain a mixed sugar solution containing sucrose microspheres;
s5, crystallization: and (3) transferring 20 parts by weight of the mixed sugar solution containing the sucrose microspheres obtained in the step (S4) into a round-bottom flask, placing the round-bottom flask in an ice bath condition, controlling the ice bath temperature to be 2 ℃, carrying out low-temperature rapid crystallization for 30min at the rotating speed of 600r/min, filtering, and drying the crystal in a baking oven at the temperature of 60 ℃ for 10h to obtain the microsphere inclusion.
The organic acid is alpha-linolenic acid.
Example 4
Substantially the same as in example 1, the only difference is that:
the preparation method of the microsphere inclusion comprises the following steps:
s1, preparing a sucrose supersaturated solution: adding 92 parts by weight of sucrose into 40 parts by weight of water, and stirring at 26 ℃ for 20 minutes at a rotating speed of 600r/min to form a sucrose supersaturated solution;
s2, ultrasonic treatment: carrying out ultrasonic treatment on the sucrose supersaturated solution obtained in the step S1 for 30min, wherein the ultrasonic temperature is controlled at 26 ℃, the ultrasonic power is 100W, and the ultrasonic frequency is 25kHz, so as to obtain the sucrose supersaturated solution after ultrasonic treatment;
s3, removing cotton sugar: adding 0.2 part of alpha-galactosidase into 30 parts of the supersaturated sucrose solution obtained in the step S2 after ultrasonic treatment, and stirring for 20min at 26 ℃ and a rotating speed of 600r/min to obtain a supersaturated sucrose solution after removing the raffinose;
s4, forming sucrose microspheres: adding 2 parts by weight of epichlorohydrin into 25 parts by weight of supersaturated sucrose solution obtained in the step S3 after removing the raffinose, and stirring for 10min at a rotating speed of 300r/min to form a water phase A; adding 3 parts of span 80 into 5 parts of liquid paraffin, and stirring at a rotating speed of 300r/min for 20min to obtain an oil phase B; dropwise adding 0.2 part of organic acid and 5 parts of oil phase B into 25 parts of water phase A at a rate of 1 drop/second respectively, stirring at 40 ℃ and a rotating speed of 900r/min for 2 hours to form uniform emulsion C, adding 1 part of glutaraldehyde into 30 parts of emulsion C, and standing at 40 ℃ for 2 hours to obtain a mixed sugar solution containing sucrose microspheres;
s5, crystallizing; and (3) transferring 20 parts by weight of the mixed sugar solution containing the sucrose microspheres obtained in the step (S4) into a round-bottom flask, placing the round-bottom flask in an ice bath condition, controlling the ice bath temperature to be 2 ℃, carrying out low-temperature rapid crystallization for 30min at the rotating speed of 600r/min, filtering, and drying the crystal in a baking oven at the temperature of 60 ℃ for 10h to obtain the microsphere inclusion.
The organic acid is a mixture of citric acid and alpha-linolenic acid according to the mass ratio of 1:1.2.
Example 5
The preparation method of the laundry effervescent tablet comprises the following steps:
according to parts by weight, 30 parts of washing particles, 3.5 parts of disintegrating agent, 0.5 part of enzyme, 40 parts of effervescent agent and 20 parts of adhesive are stirred for 30 minutes at a rotating speed of 300r/min, uniformly mixed, and then extruded on a die to form a sheet with a diameter of 2cm and a thickness of 0.5cm, so that the washing effervescent tablet is obtained.
The disintegrating agent is croscarmellose sodium.
The enzyme is alkaline protease.
The effervescent agent is prepared by mixing sodium bicarbonate and tartaric acid according to a mass ratio of 1:1.
The adhesive is absolute ethyl alcohol.
The preparation method of the washing particles comprises the following steps:
(1) Adding 20 parts of sodium dodecyl benzene sulfonate and 20 parts of sodium laureth sulfate into 100 parts of water, heating to 85 ℃, and stirring at 600r/min for 30min to obtain a mixed solution A;
(2) According to parts by weight, when 100 parts of the mixed solution A obtained in the step (1) is naturally cooled to 35 ℃, 4 parts of sodium stearate, 5 parts of glycerol cocoate and 2 parts of sodium chloride are added, the temperature is kept at 35 ℃ and the rotation speed is 600r/min, and stirring is carried out for 40min, so as to obtain a mixed solution B;
(3) Granulating the mixed solution B obtained in the step (2) by a spray granulator to obtain particles with the particle size of 0.2mm, and then placing the particles in a 60 ℃ oven for drying for 10 hours to obtain washing particles;
example 6
The preparation method of the laundry effervescent tablet comprises the following steps:
according to parts by weight, 30 parts of washing particles, 6 parts of microsphere inclusion, 2.5 parts of sterilization preservative, 3.5 parts of disintegrating agent, 0.5 part of enzyme, 40 parts of effervescent agent and 20 parts of adhesive are stirred for 30 minutes at a rotating speed of 300r/min, uniformly mixed, and then extruded on a die to form a sheet with a diameter of 2cm and a thickness of 0.5cm, so that the laundry effervescent tablet is obtained.
The disintegrating agent is croscarmellose sodium.
The enzyme is alkaline protease.
The effervescent agent is prepared by mixing sodium bicarbonate and tartaric acid according to a mass ratio of 1:1.
The adhesive is absolute ethyl alcohol.
The preparation method of the washing particles comprises the following steps:
(1) Adding 20 parts of sodium dodecyl benzene sulfonate and 20 parts of sodium laureth sulfate into 100 parts of water, heating to 85 ℃, and stirring at 600r/min for 30min to obtain a mixed solution A;
(2) According to parts by weight, when 100 parts of the mixed solution A obtained in the step (1) is naturally cooled to 35 ℃, 4 parts of sodium stearate, 5 parts of glycerol cocoate and 2 parts of sodium chloride are added, the temperature is kept at 35 ℃ and the rotation speed is 600r/min, and stirring is carried out for 40min, so as to obtain a mixed solution B;
(3) Granulating the mixed solution B obtained in the step (2) by a spray granulator to obtain particles with the particle size of 0.2mm, and then placing the particles in a 60 ℃ oven for drying for 10 hours to obtain the washing particles.
The preparation method of the microsphere inclusion comprises the following steps:
s1, preparing a sucrose supersaturated solution: adding 92 parts by weight of sucrose into 40 parts by weight of water, and stirring at 26 ℃ for 20 minutes at a rotating speed of 600r/min to form a sucrose supersaturated solution;
s2, ultrasonic treatment: carrying out ultrasonic treatment on the sucrose supersaturated solution obtained in the step S1 for 30min, wherein the ultrasonic temperature is controlled at 26 ℃, the ultrasonic power is 100W, and the ultrasonic frequency is 25kHz, so as to obtain the sucrose supersaturated solution after ultrasonic treatment;
s3, removing cotton sugar: adding 0.2 part of alpha-galactosidase into 30 parts of the supersaturated sucrose solution obtained in the step S2 after ultrasonic treatment, and stirring for 20min at 26 ℃ and a rotating speed of 600r/min to obtain a supersaturated sucrose solution after removing the raffinose;
s4, forming sucrose microspheres: adding 2 parts by weight of epichlorohydrin into 25 parts by weight of supersaturated sucrose solution obtained in the step S3 after removing the raffinose, and stirring for 10min at a rotating speed of 300r/min to form a water phase A; adding 3 parts of span 80 into 5 parts of liquid paraffin, and stirring at a rotating speed of 300r/min for 20min to obtain an oil phase B; dropwise adding 0.2 part of organic acid and 5 parts of oil phase B into 25 parts of water phase A at a rate of 1 drop/second respectively, stirring at 40 ℃ and a rotating speed of 900r/min for 2 hours to form uniform emulsion C, adding 1 part of glutaraldehyde into 30 parts of emulsion C, and standing at 40 ℃ for 2 hours to obtain a mixed sugar solution containing sucrose microspheres;
s5, crystallizing; and (3) transferring 20 parts by weight of the mixed sugar solution containing the sucrose microspheres obtained in the step (S4) into a round-bottom flask, placing the round-bottom flask in an ice bath condition, controlling the ice bath temperature to be 2 ℃, carrying out low-temperature rapid crystallization for 30min at the rotating speed of 600r/min, filtering, and drying the crystal in a baking oven at the temperature of 60 ℃ for 10h to obtain the microsphere inclusion.
The organic acid is a mixture of citric acid and alpha-linolenic acid according to the mass ratio of 1:1.2.
The sterilizing preservative is prepared by mixing inorganic sterilizing substances with dodecyl dimethyl benzyl ammonium chloride (CAS: 139-07-1) according to a mass ratio of 5:3. The inorganic bactericide is nano zinc oxide (particle size 50 nm). According to the method for evaluating the antibacterial and bacteriostatic effects of QB/T2738-2012 daily chemical products, the antibacterial effects (test strains: escherichia coli ATCC 8739, candida albicans ATCC 10231 and action time 1.5 h) of the laundry effervescent tablets prepared in example 6 are evaluated, wherein the escherichia coli sterilization rate is 91% and the candida albicans sterilization rate is 90%.
Example 7
The preparation method of the laundry effervescent tablet comprises the following steps:
according to parts by weight, 30 parts of washing particles, 6 parts of microsphere inclusion, 2.5 parts of sterilization preservative, 3.5 parts of disintegrating agent, 0.5 part of enzyme, 40 parts of effervescent agent and 20 parts of adhesive are stirred for 30 minutes at a rotating speed of 300r/min, uniformly mixed, and then extruded on a die to form a sheet with a diameter of 2cm and a thickness of 0.5cm, so that the laundry effervescent tablet is obtained.
The disintegrating agent is croscarmellose sodium.
The enzyme is alkaline protease.
The effervescent agent is prepared by mixing sodium bicarbonate and tartaric acid according to a mass ratio of 1:1.
The adhesive is absolute ethyl alcohol.
The preparation method of the washing particles comprises the following steps:
(1) Adding 20 parts of sodium dodecyl benzene sulfonate and 20 parts of sodium laureth sulfate into 100 parts of water, heating to 85 ℃, and stirring at 600r/min for 30min to obtain a mixed solution A;
(2) According to parts by weight, when 100 parts of the mixed solution A obtained in the step (1) is naturally cooled to 35 ℃, 4 parts of sodium stearate, 5 parts of glycerol cocoate and 2 parts of sodium chloride are added, the temperature is kept at 35 ℃ and the rotation speed is 600r/min, and stirring is carried out for 40min, so as to obtain a mixed solution B;
(3) Granulating the mixed solution B obtained in the step (2) by a spray granulator to obtain particles with the particle size of 0.2mm, and then placing the particles in a 60 ℃ oven for drying for 10 hours to obtain the washing particles.
The preparation method of the microsphere inclusion comprises the following steps:
s1, preparing a sucrose supersaturated solution: adding 92 parts by weight of sucrose into 40 parts by weight of water, and stirring at 26 ℃ for 20 minutes at a rotating speed of 600r/min to form a sucrose supersaturated solution;
s2, ultrasonic treatment: carrying out ultrasonic treatment on the sucrose supersaturated solution obtained in the step S1 for 30min, wherein the ultrasonic temperature is controlled at 26 ℃, the ultrasonic power is 100W, and the ultrasonic frequency is 25kHz, so as to obtain the sucrose supersaturated solution after ultrasonic treatment;
s3, removing cotton sugar: adding 0.2 part of alpha-galactosidase into 30 parts of the supersaturated sucrose solution obtained in the step S2 after ultrasonic treatment, and stirring for 20min at 26 ℃ and a rotating speed of 600r/min to obtain a supersaturated sucrose solution after removing the raffinose;
s4, forming sucrose microspheres: adding 2 parts by weight of epichlorohydrin into 25 parts by weight of supersaturated sucrose solution obtained in the step S3 after removing the raffinose, and stirring for 10min at a rotating speed of 300r/min to form a water phase A; adding 3 parts of span 80 into 5 parts of liquid paraffin, and stirring at a rotating speed of 300r/min for 20min to obtain an oil phase B; dropwise adding 0.2 part of organic acid and 5 parts of oil phase B into 25 parts of water phase A at a rate of 1 drop/second respectively, stirring at 40 ℃ and a rotating speed of 900r/min for 2 hours to form uniform emulsion C, adding 1 part of glutaraldehyde into 30 parts of emulsion C, and standing at 40 ℃ for 2 hours to obtain a mixed sugar solution containing sucrose microspheres;
s5, crystallizing; and (3) transferring 20 parts by weight of the mixed sugar solution containing the sucrose microspheres obtained in the step (S4) into a round-bottom flask, placing the round-bottom flask in an ice bath condition, controlling the ice bath temperature to be 2 ℃, carrying out low-temperature rapid crystallization for 30min at the rotating speed of 600r/min, filtering, and drying the crystal in a baking oven at the temperature of 60 ℃ for 10h to obtain the microsphere inclusion.
The organic acid is a mixture of citric acid and alpha-linolenic acid according to the mass ratio of 1:1.2.
The sterilizing preservative is prepared by mixing inorganic sterilizing substances with dodecyl dimethyl benzyl ammonium chloride (CAS: 139-07-1) according to a mass ratio of 5:3.
The preparation method of the inorganic bactericide comprises the following steps:
adding 5 parts of sodium hydroxide into 100 parts of mixed alcohol by weight for ultrasonic treatment for 15min, wherein the ultrasonic temperature is controlled at 45 ℃, the ultrasonic power is 100W, and the ultrasonic frequency is 25kHz, so as to obtain sodium hydroxide alcohol solution; adding 3.5 parts of zinc oxalate dihydrate into 200 parts of mixed alcohol, and performing ultrasonic treatment for 30min, wherein the ultrasonic temperature is controlled at 45 ℃, the ultrasonic power is 100W, and the ultrasonic frequency is 25kHz; then 25 parts of the sodium hydroxide alcohol solution is dripped, and the dripping speed is controlled at 2mL/min; after the dripping is finished, adding 0.2 part of 3-glycidoxypropyl trimethoxysilane (CAS: 2530-83-8), continuing ultrasonic treatment for 10min, centrifuging, taking precipitate, washing with water, and drying in a 60 ℃ oven for 10h to obtain an inorganic bactericide; the mixed alcohol is a mixture of ethanol and glycol according to the mass ratio of 13 (1-2). According to the method for evaluating the antibacterial and bacteriostatic effects of QB/T2738-2012 daily chemical products, the antibacterial effects (test strains: escherichia coli ATCC 8739, candida albicans ATCC 10231 and action time 1.5 h) of the laundry effervescent tablets prepared in example 7 are evaluated, wherein the escherichia coli sterilization rate is 99% and the candida albicans sterilization rate is 97%.
Test example 1
The laundry effervescent tablet in the example is subjected to anti-dyeing test, and the test standard adopts GB/T33283-2016 "fastness to industrial washing for textile color fastness test".
The preparation method of the sample comprises the following steps: in each example, a piece of black sample cloth with the color fastness of 1 and a piece of white sample cloth with the color fastness of 1 are respectively taken, the two pieces of sample cloth are cut into samples with the size of 80mm multiplied by 160mm, 25 standard stainless steel balls are placed between the two pieces of sample cloth, and the periphery of the sample cloth is sewed to obtain standard sample cloth.
The washing mode is as follows: placing a standard sample in a specified washing machine, adding the washing effervescent tablet in the embodiment of the invention for washing, wherein the washing temperature is 92 ℃, the heating rate is 1.5 ℃/min, the washing time is 60min, and drying after washing. Whiteness values of the white cloths before and after washing were measured with a whiteness meter, K/S values of the black cloths before and after washing were measured with an electronic computer color measuring and matching meter, and the test results are shown in Table 1.
Table 1: anti-staining test
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The microsphere skeleton has a certain electrostatic adsorption effect on free pigment particles, and after the microsphere skeleton wraps organic acid, citric acid can help the washing liquid to adjust the pH value, so that the adsorption effect of the microsphere skeleton is enhanced, and meanwhile, citric acid helps to dredge the pore structure of the microsphere skeleton and increase the average pore diameter; the alpha-linolenic acid can help the clothes to protect the color, reduce the damage of the polarity of water to the intermolecular action of the dye, increase the fixation of the dye on the surface of the fabric, reduce the dropping of the color of the fabric, and the citric acid and the alpha-linolenic acid are compounded, so that the dropped free pigment is adsorbed while the fading of the dye is reduced as much as possible; the microsphere skeleton coated with the organic acid is rapidly crystallized through sucrose, and further coated with the sucrose crystal, so that the organic acid can be protected from being reacted by the effervescent agent to a greater extent, after the effervescent tablet is dissolved, the sucrose crystal is released after the acid source and the alkali source in the effervescent agent react, and meanwhile, the microsphere skeleton and the coated organic acid can be protected to a greater extent after the sucrose crystal is slightly dissolved, so that the microsphere skeleton and the coated organic acid can play a role in the subsequent washing process.
Test example 2
The detergency test was carried out on the laundry effervescent tablets in examples, the test standard adopted GB/T13174-2021 for determining detergency and cycle washing Performance of detergents for clothing, 20 pieces of 10cm x 20cm Standard dirty cloth JB-01 were adopted in each example, 20 pieces of 10cm x 20cm Standard dirty cloth JB-01 were divided into A, B groups, group A used the laundry effervescent tablets in the examples of the present invention, group B used Standard detergents, both groups of samples were washed by the washing methods specified in the test standard, and the average whiteness values F of groups A and B were measured by whiteness instrument before washing, respectively A1 、F B1 Measuring average whiteness values F of the A group and the B group respectively by a whiteness meter after washing A2 、F B2 With the formula p= (F A2 -F A1 )/(F B2 -F B1 ) The decontamination ratio was calculated and the test results are shown in table 2.
Table 2: detergency test
| Decontamination ratio P | |
| Example 1 | 2.2 |
| Example 2 | 2.4 |
| Example 3 | 2.4 |
| Example 4 | 2.5 |
| Example 5 | 1.8 |
Note that: when P is more than or equal to 1.0, the conclusion is that the detergency of the sample to JB-01 sewage is equal to or better than that of a standard detergent.
In the embodiment 1, a microsphere framework is added, so that the microsphere framework can help to protect the activity of enzymes in the laundry effervescent tablet, and the detergency of the laundry effervescent tablet is obviously improved; in the forming process of the microsphere packages, the sucrose crystals further package the microsphere frameworks, so that the formed microsphere frameworks are more stable, and the decontamination capability is further improved; in the embodiment 4, the mixture of citric acid and alpha-linolenic acid according to the mass ratio of 1:1.2 is added in the process of rapidly crystallizing microsphere inclusion, so that the decontamination effect of organic acid on the effervescent tablet is improved to a certain extent.
Claims (10)
1. The laundry effervescent tablet is characterized by comprising the following raw materials in parts by weight: 20 to 40 parts of washing particles, 4 to 8 parts of microsphere inclusion, 1 to 4 parts of sterilizing preservative, 0.5 to 5 parts of disintegrating agent, 0.4 to 0.6 part of enzyme, 30 to 50 parts of effervescent agent and 15 to 25 parts of adhesive.
2. The laundry effervescent tablet of claim 1, wherein the sterilizing preservative is formed by mixing an inorganic sterilizing substance with dodecyl dimethyl benzyl ammonium chloride according to a mass ratio of 5 (1-3).
3. The laundry effervescent tablet of claim 2, characterized in that the method for preparing the inorganic bactericidal comprises the steps of:
adding 2-5 parts of sodium hydroxide into 80-100 parts of mixed alcohol according to parts by weight, and performing ultrasonic treatment for 10-20 min, wherein the ultrasonic temperature is controlled at 30-50 ℃, the ultrasonic power is 100-300W, and the ultrasonic frequency is 20-40 kHz, so as to obtain sodium hydroxide alcohol solution; adding 2-4 parts of zinc oxalate dihydrate into 150-200 parts of mixed alcohol, and performing ultrasonic treatment for 30-50 min, wherein the ultrasonic temperature is controlled at 30-50 ℃, the ultrasonic power is 100-300W, and the ultrasonic frequency is 20-40 kHz; then 20-30 parts of the sodium hydroxide alcohol solution is dripped, and the dripping speed is controlled to be 1-2 mL/min; after the dripping is finished, adding 0.1 to 0.3 part of 3-glycidoxypropyl trimethoxy silane, continuing to carry out ultrasonic treatment for 10 to 20 minutes, centrifuging, taking precipitate, washing with water, and drying in an oven at 60 to 80 ℃ for 7 to 10 hours to obtain an inorganic bactericide; the mixed alcohol is a mixture of ethanol and glycol according to the mass ratio of 13 (1-2).
4. A laundry effervescent tablet as claimed in claim 1, wherein the process for preparing the laundry particles comprises the steps of:
(1) Adding 10-25 parts by weight of sodium dodecyl benzene sulfonate and 10-25 parts by weight of sodium laureth sulfate into 60-120 parts by weight of water, heating to 75-90 ℃, and stirring for 20-40 min at a rotating speed of 500-700 r/min to obtain a mixed solution A;
(2) According to parts by weight, when 80-120 parts of the mixed solution A obtained in the step (1) is naturally cooled to 30-40 ℃, 3-5 parts of sodium stearate, 4-6 parts of glycerol cocoate and 1-3 parts of sodium chloride are added, the temperature is kept at 30-40 ℃ and the rotation speed is 500-700 r/min, and stirring is carried out for 30-50 min, so as to obtain a mixed solution B;
(3) Granulating the mixed solution B obtained in the step (2) by a spray granulator to obtain particles with the particle size of 0.1-0.3 mm, and drying the particles for 8-12 h at the temperature of 50-70 ℃ by an oven to obtain the washing particles.
5. The laundry effervescent tablet of claim 1, wherein the microsphere inclusion is prepared by a process comprising the steps of:
s1, preparing a sucrose supersaturated solution: adding sucrose into water according to parts by weight, wherein the dissolution temperature is 20-80 ℃, stirring for 15-30 min at the rotation speed of 500-700 r/min to form a sucrose supersaturated solution, and determining the solubility of the sucrose and the water at the selected dissolution temperature according to the mass ratio of the sucrose to the water to prepare the sucrose supersaturated solution with the supersaturation degree of 1.06-1.1;
s2, ultrasonic treatment: carrying out ultrasonic treatment on the sucrose supersaturated solution obtained in the step S1 for 20-40 min, wherein the ultrasonic temperature is controlled to be 20-80 ℃, the ultrasonic power is 80-120W, and the ultrasonic frequency is 20-40 kHz, so as to obtain the sucrose supersaturated solution after ultrasonic treatment;
s3, removing cotton sugar: adding 0.1-0.3 part of alpha-galactosidase into 20-40 parts of supersaturated sucrose solution obtained in the step S2 after ultrasonic treatment, stirring for 15-30 min at the temperature of 20-80 ℃ and the rotating speed of 500-700 r/min to obtain supersaturated sucrose solution after removing raffinose;
s4, forming sucrose microspheres: adding 1-3 parts by weight of epichlorohydrin into 20-30 parts by weight of supersaturated sucrose solution obtained in the step S3 after removing the raffinose, and stirring for 8-12 min at a rotating speed of 200-400 r/min to form a water phase A; adding 2-4 parts of span 80 into 4-6 parts of liquid paraffin, and stirring for 15-25 min at a rotating speed of 200-400 r/min to obtain an oil phase B; dripping 0.1-0.3 part of organic acid and 4-6 parts of oil phase B into 20-30 parts of water phase A at the speed of 1 drop/second respectively, stirring at the temperature of 35-50 ℃ and the rotating speed of 800-1000 r/min for 1.5-3.0 h to form uniform emulsion C, adding 0.5-1.5 parts of glutaraldehyde into 20-35 parts of emulsion C, and standing at the temperature of 35-50 ℃ for 1-3 h to obtain a mixed sugar solution containing sucrose microspheres;
s5, crystallizing; and (3) transferring 15-25 parts by weight of the mixed sugar solution containing the sucrose microspheres obtained in the step (S4) into a round-bottom flask, placing the round-bottom flask in an ice bath condition, controlling the ice bath temperature to be 0-2 ℃, carrying out low-temperature rapid crystallization for 20-40 min at the rotating speed of 500-700 r/min, filtering, and drying the crystal in an oven at 50-70 ℃ for 6-10 h to obtain the microsphere inclusion.
6. The laundry effervescent tablet of claim 5, wherein the organic acid is at least one of citric acid, alpha-linolenic acid, stearidonic acid, eicosapentaenoic acid, conjugated linoleic acid, gamma-linoleic acid, arachidonic acid, oleic acid, trans-oleic acid, eicosenoic acid, erucic acid, and nervonic acid.
7. The laundry effervescent tablet of claim 1, wherein the disintegrant is a mixture of one or more of croscarmellose sodium, crospovidone, starch, sodium carboxymethyl starch, hydroxypropyl starch, low substituted hydroxypropyl cellulose; the enzyme is one or more of alkaline protease, pectase, cellulase, lipase and catalase.
8. The laundry effervescent tablet of claim 1, wherein the effervescent agent is a mixture of an acid source and an alkali source; the acid source is one or a mixture of more of citric acid, malic acid, boric acid, tartaric acid, fumaric acid and inorganic mineral acid; the alkali source is sodium bicarbonate or sodium carbonate or a mixture of the two.
9. A process for the preparation of laundry effervescent tablets as claimed in any one of claims 1 to 8, characterised in that it comprises the steps of: according to parts by weight, 20 to 40 parts of washing particles, 4 to 8 parts of microsphere inclusion, 1 to 4 parts of sterilizing preservative, 0.5 to 5 parts of disintegrating agent, 0.4 to 0.6 part of enzyme, 30 to 50 parts of effervescent agent and 15 to 25 parts of adhesive are mixed at a rotating speed of 200 to 400r/min and stirred for 20 to 40min, and then extruded into a sheet on a die, so that the laundry effervescent tablet is obtained.
10. The preparation method of the microsphere inclusion is characterized by comprising the following steps of:
s1, preparing a sucrose supersaturated solution: adding sucrose into water according to parts by weight, wherein the dissolution temperature is 20-80 ℃, stirring for 15-30 min at the rotation speed of 500-700 r/min to form a sucrose supersaturated solution, and determining the solubility of the sucrose and the water at the selected dissolution temperature according to the mass ratio of the sucrose to the water to prepare the sucrose supersaturated solution with the supersaturation degree of 1.06-1.1;
s2, ultrasonic treatment: carrying out ultrasonic treatment on the sucrose supersaturated solution obtained in the step S1 for 20-40 min, wherein the ultrasonic temperature is controlled to be 20-80 ℃, the ultrasonic power is 80-120W, and the ultrasonic frequency is 20-40 kHz, so as to obtain the sucrose supersaturated solution after ultrasonic treatment;
s3, removing cotton sugar: adding 0.1-0.3 part of alpha-galactosidase into 20-40 parts of supersaturated sucrose solution obtained in the step S2 after ultrasonic treatment, stirring for 15-30 min at the temperature of 20-80 ℃ and the rotating speed of 500-700 r/min to obtain supersaturated sucrose solution after removing raffinose;
s4, forming sucrose microspheres: adding 1-3 parts by weight of epichlorohydrin into 20-30 parts by weight of supersaturated sucrose solution obtained in the step S3 after removing the raffinose, and stirring for 8-12 min at a rotating speed of 200-400 r/min to form a water phase A; adding 2-4 parts of span 80 into 4-6 parts of liquid paraffin, and stirring for 15-25 min at a rotating speed of 200-400 r/min to obtain an oil phase B; dripping 0.1-0.3 part of organic acid and 4-6 parts of oil phase B into 20-30 parts of water phase A at the speed of 1 drop/second respectively, stirring at the temperature of 35-50 ℃ and the rotating speed of 800-1000 r/min for 1.5-3.0 h to form uniform emulsion C, adding 0.5-1.5 parts of glutaraldehyde into 20-35 parts of emulsion C, and standing at the temperature of 35-50 ℃ for 1-3 h to obtain a mixed sugar solution containing sucrose microspheres;
s5, crystallizing; transferring 15-25 parts by weight of the mixed sugar solution containing the sucrose microspheres obtained in the step S4 into a round-bottom flask, placing the round-bottom flask in an ice bath condition, controlling the ice bath temperature to be 0-2 ℃, carrying out low-temperature rapid crystallization for 20-40 min at the rotating speed of 500-700 r/min, filtering, and drying the crystal in an oven at 50-70 ℃ for 6-10 h to obtain microsphere inclusion;
the organic acid is at least one of citric acid, alpha-linolenic acid, stearidonic acid, eicosapentaenoic acid, conjugated linoleic acid, gamma-linoleic acid, arachidonic acid, oleic acid, trans-oleic acid, eicosenoic acid, erucic acid and nervonic acid.
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